RO111149B1 - Active biologic extracts from plants and preparation processes therefor - Google Patents

Abstract

The invention relates to extracts biologically active, from Umbellifer seeds, with synergistic action for natural pyrethrins, pyrethroids synthesis and organophosphorus insecticides, action insecticidal and bactericidal and has a density of 0.670 ... 0,965; n20D: 1.3750 ... 1.5350; 5 ... 10% limonene; 10 ... 20% carvone; 50 ... 60% anethole; under 1% other components such as a - pinene, linalool etc. The process of obtaining them consists in that an extraction is carried out by maintaining a suspensions of plant seeds in the family umbelifers, in water or organic solvents, of ipi aliphatic hydrocarbons, petroleum fractions, alcohols, the seed / solvent ratio being 1/3 to 1/4, in an ultrasonic generating bath with a frequency between 20 and 40 KHz, for 10 ... 60 min, at ambient temperature and atmospheric pressure

Description

The present invention relates to biologically active extracts, from plants, and to a process for obtaining them, from the seeds of plants of the umbeliferous family (dill and fennel), used as synergists and / or insecticides.

It is known that pyrethrum flower extracts have an insecticidal effect, these being the first natural insecticides widely used. On the other hand, it has been observed that pyrethrum extracts from sesame oil have a more pronounced biological activity than that corresponding to the content of active substances. Thus, a number of active principles of synergistic nature for insecticides have been isolated.

It is also known that the active ingredients obtained from spontaneous or cultivated flora, used in many fields, from pharmaceuticals and pesticides to food additives, have the advantage of a minimal toxicity impact, which can be extracted by the following techniques: water vapor drive to obtain volatile oils, simple maceration, percolation, continuous extraction in Soxhlet type extractor.

These techniques have the disadvantages that the extraction of the biologically active principles is performed non-selectively, requiring long extraction times and high temperatures that can destroy some of the existing biological principles and require complicated techniques for the subsequent separation of the extracts.

The biologically active extracts, from the seeds of umbellifers, according to the invention, remove the above disadvantages, in that they have synergistic action for natural pyrethroids, synthetic pyrethroids and organophosphorus insecticides, insecticidal and bactericidal action and have: density 0.670 ... 0.965 ² % 1.3750 ... 1.5359, 5 ... 10% limonene, 10 ... 20% carvon, 50 ... 60% anetole; less than 1% other components like a - pinen, linalool.

The biologically active extracts, according to the invention, can be obtained from dill seeds, having: density 0.670 ... 0.750 and n ^ o 1.3750 ... 1.3950 or from phenolic seeds: density 0.960

... 0.965; n ² % 1,520 ... 1,535 and 1 ... 5% lemon.

The process of obtaining biologically active extracts, according to the invention, removes the disadvantages of the techniques known so far, in that the extraction is performed by maintaining a suspension of plant seeds from the LJmbeliferae family in water or organic solvents such as aliphatic hydrocarbons, oil fractions, alcohols, the seed / solvent ratio being from 1/3 to 1/4 in an ultrasonic generator bath with a frequency between 20 and 40 KHz for 10 ... 60 min, at ambient temperature and atmospheric pressure.

By applying the invention, the following advantages are obtained:

- high selectivity of extraction of biologically active principles, from accessible plants, in current culture is ensured;

- the speed of extraction is ensured by the use of ultrasounds, with an extraction time of 10 to 60 minutes compared to 10 ... 20 h, in the case of the classic extraction techniques;

- low extraction temperatures are ensured which avoids the decomposition of the components;

- the amount of solvent used is reduced;

- the active principles obtained have a low toxicity and a much smaller impact on the environment.

Three examples of embodiments of the invention are given below.

Example 1. Suspend 100 g of dill seed in 250 hexane in an Erlenmayer beaker. They are exposed for 30 minutes to ultrasound on a Quarck type ultrasonic bath with a frequency of 25 KHz (200 W). Filter, then the liquid is concentrated to 10 g.

It is analyzed by gas chromatography, coupled with mass spectroscopy, identifying several components. Of these in larger quantities are lemonade and caravan. HPLC found 7.98% limonene and 10.64% carbone.

The product is presented as a yellow - green liquid with a density

RO 111149 Bl d = 0.673 and refractive index n ² % = 1.3790.

Example 2. Suspend 100 g of dill seeds in 250 g of water in an Erlenmayer beaker. They are subjected to the action of 5 ultrasounds, as in example 1, for 60 min. Filter, then the liquid is concentrated to 10 g.

An extract with the following characteristics is obtained: density d = 0,671; n ²⁰ D: 1.3840; lemon content: 6.5%; carbon content: 10.5%.

Example 3. 100 g of phenolic seeds are suspended in 250 ml of ethyl alcohol and exposed to the action of ultrasound 15 for 30 minutes. Filter, then the liquid is concentrated to 10 g.

An extract with the following characteristics is obtained: d = 0.960; n ² % = 1,5200; main component: anetol, limonen, linalool.

Tests. The extract of dill seeds was tested for synergism by the toxic film method with the Tribolium confusum test. The results of the mixtures of dill extract + Sumialpha are presented in table 1. It is observed that all the samples have a pronounced synergistic effect (CCM »200).

Table 1

Cotoxicity coefficient (CCM) for the mixture Dill extract 30 + Technical sumialpha 84.5

The product proportion The equation of the regression line DL 50 ng / cm ² DL 90 ng / cm ² Dill extract 30 - y = -0.079 + 2.10 x 262 250 1067190 Technical sumialpha 84.5 - y = 3.97 + 5.33 x 1.55 2.7034 Dill extract + Sumialpha teh. 84.5 1/9 y = 4.3143 + 3.3906 x 1.5931 3.8003 Dill extract + Sumialpha th. 84.5 3/7 y = 4.07 + 2.23 x 2.5941 9.6871 Dill extract + Sumialpha th. 84.5 5/5 y = 4.10 + 1.50 x 3.9467 27.9332 Dill extract + Sumialpha th. 84.5 7/3 y = 4.26 + 1.78 x 2.5768 13.4264 Dill extract + Sumialpha th. 84.5 9/1 T y = 4.10 + 1.48 x 4.0261 29.2374

Tests were performed on the insecticidal effect of dill extract for Musca domestica (10 cm diameter filter paper soaked with 2 ml of test substance, placed under a bell with S = 78.5 cm ² ).

Insect mortality up to 48 hours results from the average of 3 repetitions on a single test sample (Table 2).

Table 2

The insecticidal effect of dill extract

Test substance Mortality (5%) 1 h ^{3 hrs} 24 h Dill extract 60 80 100

RO 111149 Bl

Claims (4)

claims 1. Biologically active extracts from seeds of umbellifers, characterized by their synergistic action 5 for natural pyrethroids, synthetic pyrethroids and organophosphorus insecticides, insecticidal and bactericidal action and presents: density: 0.670 ... 0.965, n ^s %: 1.370. .. 1,5350, 5 ... 10% lime, 10 ... 20% carvon, 50 ... 60% anetole; less than 1% other components, such as α-pinen, linalool, etc. 2. Biologically active extract, according to claim 1, from dill seeds, characterized in that it has a density: 0.670 ... 0.750 and n ² %: 1.3750 ... 1,3950. 3. Biologically active extract, according to claim 1, of fennel seeds, characterized in that it has a density: 0.960 ... 0.965; n ^a % and 1 ... 5% lemonade. 4. Process for obtaining the biologically active extracts of claim 1, characterized in that the extraction is carried out by maintaining a suspension of plant seeds of the Umbeliferae family in water or organic solvents such as aliphatic hydrocarbons, oil fractions, alcohols, seed ratio. / solvent being between 1/3 and 1/4, in an ultrasonic generating bath, with a frequency between 20 and 40 KHz, for 10 ... 60 min, at ambient temperature and atmospheric pressure.